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Raman Investigations to Identify Corallium Rubrum in Iron Age Jewelry and Ornaments

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Raman Investigations to Identify Corallium Rubrum in Iron Age Jewelry and Ornaments minerals Article Raman Investigations to Identify Corallium rubrum in Iron Age Jewelry and Ornaments Sebastian Fürst 1,†, Katharina Müller 2,†, Liliana Gianni 2,†, Céline Paris 3,†, Ludovic Bellot-Gurlet 3,†, Christopher F.E. Pare 1,† and Ina Reiche 2,4,†,* 1 Vor- und Frühgeschichtliche Archäologie, Institut für Altertumswissenschaften, Johannes Gutenberg-Universität Mainz, Schillerstraße 11, Mainz 55116, Germany; [email protected] (S.F.); [email protected] (C.F.E.P.) 2 Sorbonne Universités, UPMC Université Paris 06, CNRS, UMR 8220, Laboratoire d‘archéologie moléculaire et structurale (LAMS), 4 Place Jussieu, 75005 Paris, France; [email protected] (K.M.); [email protected] (L.G.) 3 Sorbonne Universités, UPMC Université Paris 06, CNRS, UMR 8233, De la molécule au nano-objets: réactivité, interactions et spectroscopies (MONARIS), 4 Place Jussieu, 75005 Paris, France; [email protected] (C.P.); [email protected] (L.B.-G.) 4 Rathgen-Forschungslabor, Staatliche Museen zu Berlin-Preußischer Kulturbesitz, Schloßstraße 1 a, Berlin 14059, Germany * Correspondence: [email protected] or [email protected]; Tel.: +49-30-2664-27101 † These authors contributed equally to this work. Academic Editor: Steve Weiner Received: 31 December 2015; Accepted: 1 June 2016; Published: 15 June 2016 Abstract: During the Central European Iron Age, more specifically between 600 and 100 BC, red precious corals (Corallium rubrum) became very popular in many regions, often associated with the so-called (early) Celts. Red corals are ideally suited to investigate several key questions of Iron Age research, like trade patterns or social and economic structures. While it is fairly easy to distinguish modern C. rubrum from bone, ivory or shells, archaeologists are confronted with ancient, hence altered, artifacts. Due to ageing processes, archaeological corals lose their intensive red color and shiny surface and can easily be confused with these other light colored materials. We propose a non-destructive multi-stage approach to identify archaeological corals amongst other biominerals used as ornament during the central European Iron Age with emphasis on optical examination and mobile Raman spectroscopy. Our investigations suggest that the noticeably high amount of misidentifications or at least uncertain material declarations existing in museums or even in the literature (around 15%) could be overcome by the proposed approach. Furthermore, the range of different materials is higher than previously expected in archaeological research. This finding has implications for contemporary concepts of social structures and distribution networks during the Iron Age. Keywords: corals; shells; Raman spectroscopy; biogenic carbonates; carotenoids; polyenes; color fading; material degradation; archaeology 1. Introduction Since Neolithic [1–3] and maybe even in Paleolithic times, 30,000 years ago [4,5], the skeletons of red precious corals (Corallium rubrum (C. rubrum)) were used as jewelry and ornaments. Because of their shiny red color and their dense and hard structure, it is the most demanded coral species in the jewelry industry, which led to an intensive commercial harvesting during the 19th and early 20th century and, in the aftermath, to a decline of its stocks (e.g., [6,7]). Minerals 2016, 6, 56; doi:10.3390/min6020056 www.mdpi.com/journal/minerals Minerals 2016, 6, 56 2 of 23 Corallium rubrum is a species within the Corallium genus of the Corallidae family and belongs taxonomically to the Anthozoa class within the phylum Cnidaria (e.g., [3,8,9]). The Anthozoa class is divided into three subclasses (Octocorallia, Hexacorallia and Ceriantharia), with the first two as the most important, being determined according to their eight-fold radial symmetry, like C. rubrum, and the third subclass by hexaradial symmetry. A living specimen of C. rubrum consists of three major components: the coral polyps are embedded in a living integument called the coenenchyme, sarcosome or coenosarc, which covers an axial skeleton [1,4,10–13]. In jewelry manufacturing, though, only the calcitic skeleton is of importance, which is why the 0.2–0.3 mm-thin coenosarc is removed prior to processing [1,3]. Unpolished Corallium branches show very characteristic longitudinally-oriented grooves on their surface, as discussed in Section 3.1, deriving from large canals in the coenosarc, which connect the polyps with each other in order to transmit nutrition and information [1,4,14]. The axial skeleton of C. rubrum consists of high-magnesium calcite (HMC) of ca. 88% Ca and compositionally 12% Mg (in number of atoms) together with some minor and trace elements [13,15,16]. The organic matrix (OM) of the axial skeleton of C. rubrum basically consists of acidic proteins and sugars [12]. Additionally, the OM contains small amounts of organic pigments. The biomineralization processes were investigated in several studies (e.g., [17–19]). Allemand and Bénazet-Tambutté [15] have shown that the skeletogenic epithelium in the coenosarc is responsible for the growth of the coral colony (from a few millimeters up to 1–2 cm per year [1,11]) by secretion of calcium carbonate, while the mechanical incorporation of sclerites produced by the scleroblasts only takes place in the apical part of the coral colony, i.e., the 1-cm terminal portion of the branches. However, new investigations of Perrin et al. have shown that the absence of sclerites from the annular part must be reconsidered, as well as the notion that there is no “cement” between the sclerites [17]. The organic pigment comprises various conjugated hydrocarbon chains, which are responsible for the intense red color of the coral. However, the exact structure of these organic compounds is still the subject of discussion. Several studies suggest a coloration due to carotenoids [8,9,11,20–22]. Other works propose unmethylated polyenes [23] and unsubstituted, all trans-polyacetylenic molecules [24], respectively. Several authors think that actually, there is a mixture of pigments each belonging to the same family [25,26]. Karampelas et al. [27] and Bergamonti et al. [28] showed that partially or completely demethylated polyenes with different conjugation lengths seem to be responsible for the colors of the species of the genus Corallium and most of the marine shells, whereas the red aragonitic hydroids of the species Stylaster roseus are colored by carotenoids, similar to those found in canthaxanthin. Raman studies on mollusks and their pearls revealed at least four and up to nine pigments in the same pearl, even in homogeneously-pigmented zones [24,29]. Chain lengths ranging from 6–14 conjugated double bonds deriving from carotenoids with unmethylated polyacetylenic backbones of various conjugation lengths were reported to be responsible for the colors. The identification of C. rubrum seems to be fairly easy for modern pieces, but can be difficult for those from archaeological records. Corallium rubrum loses its intense red color and shiny surface structure due to not yet fully understood degradation processes, which is why it can easily be mistaken for light colored materials, like bone, ivory, shells or even limestone, also used for jewelry in Central Europe during prehistoric times. Moreover, the corals and other biominerals were usually used as small polished studs or pearls (average diameter of only 0.5–1 cm), which have only small, concealed surface characteristics. It is therefore not surprising that 80 years ago, many researchers did not know that white inlays could have been made from red coral. Today, however, there is a slight tendency to declare all light colored materials as C. rubrum. Attempts have repeatedly been made to identify the raw material of the frequently-encountered and today whitish jewelry inlays using different analytical methods, as for instance X-ray fluorescence (XRF) [30–32], X-ray diffraction (XRD), isotope analysis, as well as electron microprobe (EMP) [32,33], micro-computed X-ray tomography (µ-CT) [34] and Raman spectroscopy [35]. These studies help toward better knowledge of the biominerals used for the manufacturing of precious objects. Minerals 2016, 6, 56 3 of 23 Schrickel et al. [35–38] recently used micro-X-ray tomography (micro-CT), digital microscopy, full-field micro-XRF using the X-ray-color camera, Raman spectroscopy and XRD to investigate mainly late Iron Age coral ornamented fibulae (“Mitteldeutsche Korallenfibeln”) from Central Germany. Based on the MgCO3 contents and specific structural features, the authors conclude that most of the materials used to ornament the fibulae were nummulites or other Foraminifera, and not C. rubrum. During the Central European Iron Age, more specifically between 600 and 100 BC, red precious corals (C. rubrum) became very popular in many regions, often associated with the so-called (early) Celts. Red corals are ideally suited to investigate several key questions of Iron Age research [39–44]. As a prestigious long-distance trade good, C. rubrum can change the social status of a grave or site and, yet, its whole interpretation. On a macro scale, the distribution of coral finds help to gain a better understanding of trade patterns, communication routes and Iron Age social structures. It is therefore very instructive to generate an approximation of the extent of the actual use of coral and to find out which other materials have been applied as jewelry ornaments at which time. A better identification of the raw material used for the manufacturing of ancient objects
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